Process of purifying iodin



R. M'. CARTER.

i PROCESS or PURIFYJNG loom,

APPLICATION FILED DEC. 2.4, 1916.

uten'cd Dec. 9,1919,

Z SHEETSSHEETI R.M.CAR1ER. PROCESS OF PURIFYING'IODIN. APPLICAION FILED DEC 24,*1918.

Patented Dec.

2 SHEETS-SHEET 2.

#STATES PATENT OFFICE.

RAY M. CARTERQOF BALTIMORE, MARYLAND, ASSIGNOR T0 U. S. INDUSTRIAL ALCOHOL C0., A. CORPORATION OF WEST VIRGINIA.

Piaocuss or PURIFYING IoDIN.

Specification of Letters Patent.

PatentedDee. 9, 1. 19.

Application filed December 24, 1918. Serial No. 268,163.

To all whom it may concern.'

Be it known that I, RAY M. CARTER, of Baltimore, in the State of Maryland, have invented a certain new and useful Improvement in Processes of Purifying Iodin, and do hereby declare that the following is a full, clear, and exact description thereof.

My invention relates Vparticularly to a process of purifying iodin in such a manner as to remove .the impurities which are ordinarily present in the commercial product.

The object of my invention is to provide a process by means of which iodin may be purified, and particularly in such a manner as to remove the iron and other halogens present therein. Iron is present in commer cial iodin as iron iodid, and other halogens, that is chlorin and bromin, are present as iodin chlorid and iodin bromid. All of these compounds pass over with iodin when it is sublimated, in the usual process that is used for the purification of iodin. It ismy object to provide a process by meansof which iodin can be purified and in such a manner as to remove these impurities.

Further objects of my invention will appear Ifrom the' detailed description thereof contained hereinafter. Y Y

While my invention is capable of being carried out in many different ways, for the purpose of illustration I shall describe only certain ways of carrying out the samehereinafter, and while it is capable of being carried out in connection withmany differentA types of apparatus, I have shown only one type of apparatus forl use in 4connection therewith in the accompanying drawings, in which-` Figure 1' is a side elevation of an apparatus which may be used iyconnecton with my invention;

Fig. 2 is a vertical section through the vaporizin g kettle;

Fig. 3 is a plan View o f the same; y

Fig.' 4 is a horizontal section through the same; and

- LLjfor introducing a heated gas or vapor, such Fig. 5 is a; vertical section through the condenser.

In the drawings, I have shown a vaporizin kettle 1, having a removable cover 2 and a drain pipe 3. In the top of the kettle there is, furthermore, provided a valved inlet pipe as steam, by means of a perforated coil 5 lo- ,cated at the bottom of the kettle', and an outl let pipe 6 to allow the vapors of iodin, as well as the heated gas or vapor, to pass out from the kettle 1. The' kettle is, furthermore, provided with a window 7, so that the contents maybe viewed from time to time.

Into the kettle 1 I introduce 200 pounds of commercial iodin, which will contain im.

purities, such for example as ironv iodid, iodin chlorid and iodin bromd. I then introduce into the kettle a solution of'potassium iodid 'containing 10 pounds of potassium iodid and 100 pounds of `a solvent, suoli for example-as water.. The heated vgas or vapor,such for exampleas steam, together with the vapor-ized iodin, now passout of the kettle 1 by means ofthe rpipe 6.*-1`Thfe'ste`am decomposes the iron iodid in the kettle'l,

articularly. in the presence of the potassium iodid, sor that-.the iodin is liberated: therefrom` and is driven off, therefore,`with th e gaseous heating medium. T he'iodin chlorid and iodin bromid are, furthermore, decomposed by the steam, especially in the presence of the potassium iodid, so as to form potascollects above a perforated plate 14 in the bottom of the condenser 8, where it is filtered from the cohdensed Water, `which may be drawn off when desired by means of a drawof pipe 15 in the bottom of the condenser 8.

Below the perforated plate 14 there-is a vent pipe 16 entering the condenser 8, so as to exhaust accumulated uncondensed vapors for the removal of the solidified iodin which which may occur in the condenser to the outer air. Hot and cold water are supplied to the ipe 11 by means of valved supply pipes Il; and 18, respectively, and 'a drain pipe 19 conveys the eiiiu'ent from 'the pipe 12 to a sewer.-

y In the operation of1 my invention, the l iodin containing impurities acted upon by the heated gaseous medium in the kettle 1 in such a manner as to set free the'iodin from the'iron iodid.4 the iodin chlorid'and iodin bro1nid,so t1n 1t substantially tl'ie'entire quan'.

.tity vof iodin present inthe body of.1ocl iu' 'treated,.whether combined'or lincombincd,is.

' released and driven off from the kettle l and obtaineclin the-form of a solid in the Acom denser 8, from which the condensed water is tiltered oif' and removed.'

Water of the desired temperature, that is to say'of any temperature which will oondensc the iodin without freezing the lWater,

is supplied through the pipe 511, and theef fiucnt is drawn oii by the pipe l2.

. In case tllenpparatus is operatingjin such a manner as to permitiodin. vapors toaccumulate without' condensation' in the`\ condenser these vapors are vented to the o1'1t e1 V air by means of the pipe 1'6, so as notio -in-A 'jure the workmen operating the apparatus..

, The wet iodinthus. removed from the oondenser #8f isv dried in any` suitablicontainer at low temperature, as. for example t.he.tem-

perature of theatnosphere, but-with the api plication of a, highvacu'iim, as f or example 128 inches of mercury. -In this way an iodin.

is obtained which is .freed fr om'tlieV iron and other halogens ordinarily found therein.

` It-will be understood.t halt','insteadg of the" y Apotassium'-iodid, I 'may4 use sodium iodidga 'calcium iodid 'orany soiuble iodid,fand thfatg nste'a'd'of the water, `I .may nse'some lother solvent of the iodid of the' alkali or alkali earthmetal utilized. l

' While I have described 'my'.i'lifention 'above in detaiLI wish it to befunder'sto'od that many changes may be made therein without departing-from th'e's'pirit of thsame.

1. The'process which comprises subject# ing iodin containingas an impurity an iodin compound. to `the actionof a ,heatedgafseu's medium so as to liberate the iodi'n contained in said impurity-and yapo'rize the -iodnj 2. The process .which comprises subjecting Y.

iodin containing` :is anj impurity an iodincompound in the presencef asoiutoxf'of arr ingiodin ontai'n'l' purity and vap compound in" thc' .prcscncef as'sollition of 75" L iodin from .the lrcmainderof the c ondensafe tion of a heated gaseous 11'} ed1`m .'so' as to and .vaporize tl1c'iodi n. 3. The process which: comprises subjeeb vliberate the iodin con'tmnedin s ai'd impurity.'

ing'iodin containing as an 'impurity 4an idin compound t0' the-.action of alieatedgaseons mediumso as to libera' the. iodin contained in Said-impurity and veporizeth'e iodn';

thencondensing the iodin.

' f4. The process whichcompriscs subjecting' A' iodiu containing as en impurity en -india A 'compound in the presenoeiof @Isolation of an' iodio" of 'an alkali forming lx'netal'ito 'the actionof aheated-'gaseousimednun so as to liberate .the.-'iodin.contained in said 'impurity and vapori'ze the iodin end then condensingA the iodxn. 4- f; 5. The processwhxchfeomprises subjecting 12. The process` which comm-isos whim-.- ing iodin containing' as an impurity iron icdid in the presence of a solution ofxan-idid' of an'alkali'formingrnrtal in Water 11o "tire-- --action of' steam so as. to' liberate theiodii `i215 contained in'said'fimpurity'and vapori'ze' the iodin 'andV then'condcnsmg" .the iodln.

13. 'The process which comprises subject-' mg iodin .containing asanimpurxty. iron iodid'tot'he action of steam so as to liberate-139'.

u inf. .1ii""119 Lea-13761 the iodin contained in said impurity and vaporize the iodin, then condensing the iodin, andthen ltering ott the iodin from the remainder of the condensate and drying the iodin.

14. The process Which comprises subjecting iodin containing as an impurity iron iodid in the presence of a solution of an iodid ofV an alkali forming metal in Water to the action of steam so as Vto liberate the iodin contained in said impurity and vaporize the iodin, then condensing the iodin, and then filtering ofi the iodin from the remainder of the condensate and drying the iodin.

15. The process which comprises subjecting iodin containing as an impurity iron iodid to the action of steam so as to liberate the iodin contained in said impurity and vaporize the iodin, then condensing the iodin, and then filtering 0H the iodin `from the remainder of the condensate and drying the iodin at a low temperature and high vacuum. i

16. The processwhich comprises subjecting iodin. containing as an impurity iron iodid in the presence of a solution of an iodid of an alkali forming metal in Water to the action of steam so as to liberate the iodin contained in said impurity and vaporize the iodin, then condensing the iodin, and then ltering ofi' the iodin from the remainder of the condensate and drying the iodin at a low temperature and high vacuum.

17. The process which comprises subjecting iodin containing as an impurity iron iodid and a compound containing iodin and another halogen to the action of steam so as toliberate the iodin contained in said impurity and vaporize the iodin.

18. The process which comprises subjecting iodin containing as an impurity iron i iodid and a compound containing iodin and another halogen in the presence of a solution of an iodid of an alkali forming metal in Water to the action of steam so as to liberate the iodin contained i said impurity and vaporize the iodin..

19. The process which comprises subjectinnr iodin containing as an impurity iron iodid and a compound'containing iodin and another halogen to the action of steam so as to liberate the iodin contained in said impurity and vaporize the iodin and then condens'ing the iodin.

20. The process which comprises subjecting iodin containing as an impurity iron iodid and a compound containing iodm and another halogen in the presence of a solution o fan iodid of an alkali forming metal in water to the action of steam so as to liberate the iodin cpnlfirined in 'said impurity and vaporize the'lf'odin and then condensing the iodin. l

21. The process which comprises subjecting iodin containing as an impurity iron iodid and a compound containing iodin and another halogen to the action of steam so as to liberate the iodin containedin said imi water to the action of steam so as to liberate the iodin contained in said impurity and vaporize the iodin, then condensing the iodin, and. then filtering oit the iodin from the remainder of the condensate and drying the iodin. l

23. The process which comprises subjecting iodin containing as an impurity iron iodid -and a compound containing iodin and another halogen to the action of steam so as to liberate the iodin contained in said impurity and vaporize the iodin, then condensing the iodin, and then filtering ofi" the iodin from the remainder of the condensate and drying the iodin at a low temperature and high vacuum. j

24. The process which comprises subjecting iodin containing as an impurity iron iodid and a compound containing iod'm and another halogen in the presence of a solution of an iodid/of an alkali forming metal in Water to/the action of steam so as to liberato the iodin contained in said, impurity and vaporize the iodin, then condensing the iodin, and then filtering ofi' the iodin from the remainder of the condensate and drying -the lodm at a low temperature and high vacuum.

In testimony that I claim the foregoing I have hereunto set my hand.

. RAY M. CARTER. Witnesses:

ARTHUR A. BACKHAUS, WILLIAM WATSON. 

